CN103113910B - Pretreatment method for raw material of coal-based needle coke - Google Patents
Pretreatment method for raw material of coal-based needle coke Download PDFInfo
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Abstract
The invention discloses a pretreatment method for a raw material of coal-based needle coke; the method comprises the following steps of: 1) adding the raw material and diluter into a stirring kettle, separating out solvent insoluble substance; 2) pumping the mixed solution into a heating pressure filter kettle; 3) filtering the mixed solution by a filter material layer in the heating pressure filter kettle; 4) injecting inert gas into the heating pressure filter kettle, pressurizing, heating and thermally filtering under the protection of the inert gas; 5) centrifugally filtering the filtrate so as to obtain centrifugate; and 6) distilling the centrifugate at normal temperature to recover diluter, thus finally the refined purified asphalt stock used for producing coal-based needle coke is obtained. The yield of the asphalt stock used for producing coal-based needle coke obtained by the process is improved by 10-20% than that of other methods; by adopting the method, the needle coke with higher coking yield, better optical anisotropy optical tissue structure and low thermal expansion coefficient value can be obtained; and the method is simple in production process and low in equipment cost, and can easily realize large-scale production.
Description
Technical field
The present invention relates to coal tar, coal-tar pitch, return the processing technology field of joining viscid bitumen and remove quinoline insolubles (QI), specifically, is a kind of preprocessing method of raw materials of producing coal-based needle coke.
Background technology
Needle coke is the main raw material of producing superpower, ultra-high power graphite electrode, only has with the qualified refining purification viscid bitumen through special processing and makes raw material, just can produce needle coke, also only has qualified needle coke just can produce ultra-high power graphite electrode.It is needle coke and coal-based needle coke that needle coke is divided into oil according to the difference of raw material, and because oil price is high and the lighting increasingly of refining of petroleum, causing oil is that needle-shape coke raw material reduces, thereby has impelled the development of coal-based needle coke production technology.
Coal tar, coal-tar pitch and returning is joined and in viscid bitumen, is all contained a certain amount of quinoline insolubles (QI), quinoline insolubles (QI) is mainly decolorizing carbon and the coal dust bringing with coal gas from coking chamber of coke oven and the coke powder that the polycondensation of the toluene insolubles degree of depth generates, in needle coke Coking Process, quinoline insolubles (QI) can be attached to around established mesophasespherule, hinder and spherularly further grow up and merge, thereby can not generate the needle coke that fibrous texture is good.Therefore, in order to produce qualified needle coke, must and return feed coal tar, coal-tar pitch and join viscid bitumen and carry out purifying treatment, remove the detrimental impurity such as quinoline insolubles (QI) that hinders mesophase ball growth.
Remove at present coal tar, coal-tar pitch and return the method for joining quinoline insolubles in viscid bitumen (QI) and mainly contain flash method, solvent method, centrifuging and hydrogenation method.But aforesaid method exists, complex process, cost of investment are high, decontamination effect improving does not reach the shortcomings such as requirement.
Summary of the invention
The object of this invention is to provide a kind of preprocessing method of raw materials for the production of coal-based needle coke, taking coal tar, coal-tar pitch or return and join viscid bitumen as raw material, taking coal tar light component light oil or washing oil as thinner, after fully mixing, through heating and pressurizing heat filtering and centrifuging, remove coal tar, coal-tar pitch or return the quinoline insolubles (QI) of joining in viscid bitumen, then through normal pressure Distillation recovery thinner, produce refining purifying pitch, obtain being applicable to producing the raw material of coal-based needle coke.
The present invention is realized by the following technical programs.
A preprocessing method of raw materials for coal-based needle coke, comprises the steps:
1) raw material and thinner are joined in stirring tank according to mass ratio 1:1～10 ratio, after stirring, isolate solvent insolubles;
2) mixed solution of isolating in step 1) after solvent insolubles is extracted out and sent in heating and pressurizing filtration still by feedstock pump;
3) mixed solution filters the filtration material layer filtration of laying in still through heating and pressurizing;
4) filter still injecting inert gas via air intake valve to heating and pressurizing, pressurization, under protection of inert gas, filters mixed solution heating in still by heating and pressurizing, opens discharge valve, and mixed solution carries out heat filtering;
5) filtrate after step 4) heat filtering, joins in link-suspended basket centrifuge, and centrifuging, obtains centrifugate;
6) centrifugate step 5) being obtained, under the condition of certain temperature, reclaims thinner through air distillation in atmospheric distillation tower, finally obtains the refining purifying pitch raw material for the production of coal-based needle coke.
Further, in the inventive method:
Described raw material is coal tar, coal-tar pitch or returns and join viscid bitumen.
Described thinner is coal tar light component light oil or washing oil.
The filtration material layer that described heating and pressurizing is filtered in still is combined by mixture and the stainless steel filtering net of diatomite, pearlstone or diatomite and pearlstone, the granularity of diatomite and expanded perlite granule is 70～400 orders, stainless steel filtering net order number is 300～700 orders, and filtering layer thickness is 5～10 centimetres.
Described is N to heating and pressurizing filtration still injecting inert gas
2or Ar.
In described step 4), filter still to heating and pressurizing and be forced into 0.2～2MPa, mixed solution is heated to 100～200 DEG C.
In described step 5), the filter cloth order number of whizzer is 800～1300 orders, and centrifuge speed is 1000～2000 revs/min.
Centrifugate air distillation under 260～300 DEG C of conditions of temperature in described step 6).
Compared with prior art, the present invention has the following advantages:
(1) yield of the asphalt stock for the production of coal-based needle coke that this technique makes has improved 10～20% than additive method.
(2) can obtain the needle coke that coking yield is higher, optical anisotropy structure of fibrous tissue is better and Coefficient of Thermal Expansion value is little.
(3) production technique is simple, and equipment cost is low, is easy to realize scale operation.
Brief description of the drawings
Fig. 1 is the apparatus structure schematic diagram that the technique of coal-based needle coke raw materials pretreatment of the present invention is taked.
In figure: 1-stirring tank 2-feedstock pump 3-material inlet valve 4-heating and pressurizing is filtered still 5-filtration material layer 6-air intake valve 7-venting valve 8-discharge valve 9-whizzer 10-atmospheric distillation tower.
Embodiment
Below in conjunction with drawings and Examples, the present invention is described in further details.
The technique of coal-based needle coke raw materials pretreatment of the present invention takes device as shown in Figure 1 to realize, described coal-based needle coke raw material preprocessing device, comprise stirring tank 1 and pass through the interconnective heating and pressurizing of feedstock pump 2 and pipeline and stirring tank 1 and filter still 4, heating and pressurizing is filtered still 4 and is connected successively whizzer 9 and atmospheric distillation tower 10 by pipeline.Wherein, stirring tank 1 is vertical empty still, is provided with axial agitator in still, and top is provided with diluent inlet and feed(raw material)inlet, and bottom is provided with residue outlet, and the raw material at stirring tank 1 middle part is connected with the entrance of feedstock pump 2 by pipeline with the mixture export of thinner.The top of filtering still 4 in heating and pressurizing is provided with rare gas element inlet mouth and rare gas element venting port, on pipeline, be provided with air intake valve 6 near rare gas element inlet mouth place, rare gas element venting port, by tube emptying, is provided with venting valve 7 near rare gas element venting port place on pipeline.Heating and pressurizing is filtered still 4 inside and is provided with filtration material layer 5, and filtration material layer 5 is located at heating and pressurizing and filters in still 4 cavitys 1/6 place to tower top at the bottom of tower, and filtration material layer 5 is combined by solid particulate matter and stainless steel filtering net, and solid particulate matter is layered on stainless steel filtering net uniformly.The bottom that heating and pressurizing is filtered still 4 is provided with filtrate outlet, and filtrate outlet is connected with the opening for feed of whizzer 9 by pipeline, and pipeline is provided with discharge valve 8, and whizzer 9 bottoms are provided with sludge discharge tube.Atmospheric distillation tower 10 is tray column, and stage number is 30～120, and reflux ratio is 4～10.The top of atmospheric distillation tower 10 is provided with solvent outlet, solvent outlet is connected with coagulation tank and realizes the recovery of thinner with water cooler successively, the bottom of atmospheric distillation tower 10 is provided with refining purifying pitch outlet, and final, refining purifying pitch exports extraction thus for follow-up delayed coking and calcination process.
The present invention is the raw material pretreatment process method that realizes coal-based needle coke by said apparatus structure, and method comprises the steps:
1) by feed coal tar, coal-tar pitch or return and join viscid bitumen and thinner coal tar light component light oil or washing oil, join in stirring tank 1 according to mass ratio 1:1～10 ratio, after stirring, isolate solvent insolubles;
2) mixed solution of isolating in step 1) after solvent insolubles is extracted out and sent in heating and pressurizing filtration still 4 by feedstock pump 2; When the injection rate of mixed solution reach heating and pressurizing filter still 4 volumes 2/3 time, close material inlet valve 3;
3) mixed solution filters the filtration material layer filtration of laying in still 4 through heating and pressurizing; The filtration material layer that heating and pressurizing is filtered in still 4 is combined by mixture and the stainless steel filtering net of diatomite, pearlstone or diatomite and pearlstone, the mixture of diatomite or pearlstone or diatomite and pearlstone is layered on stainless steel filtering net uniformly, the granularity of diatomite and expanded perlite granule is 70～400 orders, stainless steel filtering net order number is 300～700 orders, and filtering layer thickness is 5～10 centimetres;
4) filter still 4 injecting inert gas (N via air intake valve 6 to heating and pressurizing
2or Ar), be forced into 0.2～2MPa, under protection of inert gas, heating and pressurizing is filtered to mixed solution in still 4 and be heated to 100～200 DEG C, open discharge valve 8, mixed solution carries out heat filtering, and part residual air is discharged through venting valve 7;
5) filtrate after step 4) heat filtering, joins in link-suspended basket centrifuge 9, and the filter cloth order number of whizzer is 800～1300 orders, with the rotating speed centrifuging of 1000～2000 revs/min, obtains centrifugate;
6) centrifugate step 5) being obtained is under the condition of 260～300 DEG C of temperature, interior through air distillation recovery thinner at atmospheric distillation tower 10, finally obtains the refining purifying pitch raw material for the production of coal-based needle coke.
Following embodiment is used for further illustrating different instances of the present invention.
Embodiment 1:
Feed coal tar and thinner washing oil are joined in stirring tank 1 according to mass ratio 1:1, fully mix; Mixed solution is extracted out and is sent in heating and pressurizing filtration still 4 by feedstock pump 2, the filtration material layer of wherein laying in heating and pressurizing filtration still 4 is combined by diatomite and stainless steel filtering net, the granularity of diatomite particle is 70 orders, and stainless steel filtering net order number is 300 orders, and filtering layer thickness is 5 centimetres; Then filter still 4 to heating and pressurizing and inject N
2be forced into 0.2MPa, be heated to 100 DEG C, mixed solution after heat filtering joins in link-suspended basket centrifuge 9, the filter cloth order number of whizzer is 800 orders, and with the rotating speed centrifuging of 1000 revs/min, the centrifugate obtaining air distillation at 260 DEG C goes out thinner, obtain the pitch for the production of coal-based needle coke, the content of quinoline insolubles is 0.12%.
Embodiment 2:
Feed coal pitch and thinner light oil are joined in stirring tank 1 according to mass ratio 1:1, fully mix; Mixed solution is extracted out and is sent in heating and pressurizing filtration still 4 by feedstock pump 2, the filtration material layer 5 of wherein laying in heating and pressurizing filtration still 4 is combined by pearlstone and stainless steel filtering net, the granularity of expanded perlite granule is 100 orders, stainless steel filtering net order number is 300 orders, and filtering layer thickness is 5 centimetres; Then filter still 4 to heating and pressurizing and inject N
2be forced into 0.8MPa, be heated to 180 DEG C, mixed solution after heat filtering joins in link-suspended basket centrifuge 9, the filter cloth order number of whizzer is 800 orders, and with the rotating speed centrifuging of 1000 revs/min, the centrifugate obtaining air distillation at 260 DEG C goes out thinner, obtain the pitch for the production of coal-based needle coke, the content of quinoline insolubles is 0.13%.
Embodiment 3:
Raw material is returned and joins viscid bitumen and thinner light oil joins in stirring tank 1 according to mass ratio 1:5, fully mix; Mixed solution is extracted out and is sent in heating and pressurizing filtration still 4 by feedstock pump 2, the filtration material layer 5 of wherein laying in heating and pressurizing filtration still 4 is combined by diatomite and stainless steel filtering net, the granularity of diatomite particle is 200 orders, and stainless steel filtering net order number is 700 orders, and filtering layer thickness is 7 centimetres; Then filter still 4 to heating and pressurizing and inject N2, be forced into 1MPa, be heated to 150 DEG C, mixed solution after heat filtering joins in link-suspended basket centrifuge 9, the filter cloth order number of whizzer is 1000 orders, and with the rotating speed centrifuging of 1500 revs/min, the centrifugate obtaining air distillation at 280 DEG C goes out thinner, obtain the pitch for the production of coal-based needle coke, the content of quinoline insolubles is 0.11%.
Embodiment 4:
Feed coal pitch and thinner washing oil are joined in stirring tank 1 according to mass ratio 1:5, fully mix; Mixed solution is extracted out and is sent in heating and pressurizing filtration still 4 by feedstock pump 2, the filtration material layer 5 of wherein laying in heating and pressurizing filtration still 4 is combined by mixture and the stainless steel filtering net of diatomite and pearlstone, be crushed to 150 object diatomite be crushed to 150 object pearlstones in mass ratio 1:2 mix, stainless steel filtering net order number is 500 orders, and filtering layer thickness is 8 centimetres; Then filter still 4 to heating and pressurizing and inject Ar, be forced into 2MPa, be heated to 170 DEG C, mixed solution after heat filtering joins in link-suspended basket centrifuge 9, the filter cloth order number of whizzer is 1300 orders, and with the rotating speed centrifuging of 1500 revs/min, the centrifugate obtaining air distillation at 290 DEG C goes out thinner, obtain the pitch for the production of coal-based needle coke, the content of quinoline insolubles is 0.13%.
Embodiment 5:
Feed coal tar and thinner light oil are joined in stirring tank 1 according to mass ratio 1:6, fully mix; Mixed solution is extracted out and is sent in heating and pressurizing filtration still 4 by feedstock pump 2, the filtration material layer 5 of wherein laying in heating and pressurizing filtration still 4 is combined by diatomite and stainless steel filtering net, the granularity of diatomite particle is 150 orders, and stainless steel filtering net order number is 600 orders, and filtering layer thickness is 7 centimetres; Then filter still 4 to heating and pressurizing and inject Ar, be forced into 1.2MPa, be heated to 200 DEG C, mixed solution after heat filtering joins in link-suspended basket centrifuge 9, the filter cloth order number of whizzer is 1300 orders, and with the rotating speed centrifuging of 2000 revs/min, the centrifugate obtaining air distillation at 270 DEG C goes out thinner, obtain the pitch for the production of coal-based needle coke, the content of quinoline insolubles is 0.10%.
Embodiment 6:
Raw material is returned and joins viscid bitumen and thinner washing oil joins in stirring tank 1 according to mass ratio 1:8, fully mix; Mixed solution is extracted out and is sent in heating and pressurizing filtration still 4 by feedstock pump 2, the filtration material layer 5 of wherein laying in heating and pressurizing filtration still 4 is combined by diatomite and stainless steel filtering net, the granularity of diatomite particle is 300 orders, and stainless steel filtering net order number is 700 orders, and filtering layer thickness is 10 centimetres; Then filter still 4 to heating and pressurizing and inject N
2be forced into 1.5MPa, be heated to 170 DEG C, mixed solution after heat filtering joins in link-suspended basket centrifuge 9, the filter cloth order number of whizzer is 1000 orders, and with the rotating speed centrifuging of 2000 revs/min, the centrifugate obtaining air distillation at 300 DEG C goes out thinner, obtain the pitch for the production of coal-based needle coke, the content of quinoline insolubles is 0.11%.
Embodiment 7:
Feed coal tar and thinner washing oil are joined in stirring tank 1 according to mass ratio 1:5, fully mix; Mixed solution is extracted out and is sent in heating and pressurizing filtration still 4 by feedstock pump 2, the filtration material layer 5 of wherein laying in heating and pressurizing filtration still 4 is combined by pearlstone and stainless steel filtering net, the granularity of expanded perlite granule is 200 orders, stainless steel filtering net order number is 500 orders, and filtering layer thickness is 5 centimetres; Then filter still 4 to heating and pressurizing and inject N
2be forced into 1.8MPa, be heated to 200 DEG C, mixed solution after heat filtering joins in link-suspended basket centrifuge 9, the filter cloth order number of whizzer is 1000 orders, and with the rotating speed centrifuging of 1000 revs/min, the centrifugate obtaining air distillation at 260 DEG C goes out thinner, obtain the pitch for the production of coal-based needle coke, the content of quinoline insolubles is 0.14%.
Embodiment 8:
Feed coal pitch and thinner light oil are joined in stirring tank 1 according to mass ratio 1:10, fully mix; Mixed solution is extracted out and is sent in heating and pressurizing filtration still 4 by feedstock pump 2, the filtration material layer 5 of wherein laying in heating and pressurizing filtration still 4 is combined by pearlstone and stainless steel filtering net, the granularity of expanded perlite granule is 150 orders, stainless steel filtering net order number is 700 orders, and filtering layer thickness is 10 centimetres; Then filter still 4 to heating and pressurizing and inject Ar, be forced into 2MPa, be heated to 150 DEG C, mixed solution after heat filtering joins in link-suspended basket centrifuge 9, the filter cloth order number of whizzer is 1300 orders, and with the rotating speed centrifuging of 1500 revs/min, the centrifugate obtaining air distillation at 300 DEG C goes out thinner, obtain the pitch for the production of coal-based needle coke, the content of quinoline insolubles is 0.10%.
Embodiment 9:
Feed coal tar and thinner washing oil are joined in stirring tank 1 according to mass ratio 1:5, fully mix; Mixed solution is extracted out and is sent in heating and pressurizing filtration still 4 by feedstock pump 2, the filtration material layer 5 of wherein laying in heating and pressurizing filtration still 4 is combined by mixture and the stainless steel filtering net of diatomite and pearlstone, be crushed to 70 object diatomite be crushed to 70 object pearlstones in mass ratio 1:1 mix, stainless steel filtering net order number is 600 orders, and filtering layer thickness is 6 centimetres; Then filter still 4 to heating and pressurizing and inject N
2be forced into 1.6MPa, be heated to 190 DEG C, mixed solution after heat filtering joins in link-suspended basket centrifuge 9, the filter cloth order number of whizzer is 1000 orders, and with the rotating speed centrifuging of 1800 revs/min, the centrifugate obtaining air distillation at 290 DEG C goes out thinner, obtain the pitch for the production of coal-based needle coke, the content of quinoline insolubles is 0.12%.
Embodiment 10:
Raw material is returned and joins viscid bitumen and thinner light oil joins in stirring tank 1 according to mass ratio 1:8, fully mix; Mixed solution is extracted out and is sent in heating and pressurizing filtration still 4 by feedstock pump 2, the filtration material layer 5 of wherein laying in heating and pressurizing filtration still 4 is combined by mixture and the stainless steel filtering net of diatomite and pearlstone, be crushed to 400 object diatomite be crushed to 400 object pearlstones in mass ratio 1:1 mix, stainless steel filtering net order number is 700 orders, and filtering layer thickness is 10 centimetres; Then filter still 4 to heating and pressurizing and inject Ar, be forced into 2MPa, be heated to 200 DEG C, mixed solution after heat filtering joins in link-suspended basket centrifuge 9, the filter cloth order number of whizzer is 1300 orders, and with the rotating speed centrifuging of 2000 revs/min, the centrifugate obtaining air distillation at 300 DEG C goes out thinner, obtain the pitch for the production of coal-based needle coke, the content of quinoline insolubles is 0.09%.
Above content is in conjunction with concrete preferred implementation further description made for the present invention; can not assert that the specific embodiment of the present invention only limits to this; for general technical staff of the technical field of the invention; without departing from the inventive concept of the premise; can also make some simple deduction or replace, all should be considered as belonging to the present invention and determine scope of patent protection by submitted to claims.
Claims (1)
1. a preprocessing method of raw materials for coal-based needle coke, is characterized in that, the method comprises the steps:
1) raw material and thinner are joined in stirring tank according to mass ratio 1:1～10 ratio, after stirring, isolate solvent insolubles;
2) mixed solution of isolating in step 1) after solvent insolubles is extracted out and sent in heating and pressurizing filtration still by feedstock pump;
3) mixed solution filters the filtration material layer filtration of laying in still through heating and pressurizing;
4) filter still injecting inert gas via air intake valve to heating and pressurizing, pressurization, under protection of inert gas, filters mixed solution heating in still by heating and pressurizing, opens discharge valve, and mixed solution carries out heat filtering;
5) filtrate after step 4) heat filtering, joins in link-suspended basket centrifuge, and centrifuging, obtains centrifugate;
6) centrifugate step 5) being obtained, under the condition of certain temperature, reclaims thinner through air distillation in atmospheric distillation tower, finally obtains the refining purifying pitch raw material for the production of coal-based needle coke;
Described raw material is coal tar, coal-tar pitch or returns and join viscid bitumen;
Described thinner is coal tar light component light oil or washing oil;
The filtration material layer that described heating and pressurizing is filtered in still is combined by mixture and the stainless steel filtering net of diatomite, pearlstone or diatomite and pearlstone, the granularity of diatomite and expanded perlite granule is 70～400 orders, stainless steel filtering net order number is 300～700 orders, and filtering layer thickness is 5～10 centimetres;
Described is N to heating and pressurizing filtration still injecting inert gas
2or Ar;
In described step 4), filter still to heating and pressurizing and be forced into 0.2～2MPa, mixed solution is heated to 100～200 DEG C;
In described step 5), the filter cloth order number of whizzer is 800～1300 orders, and centrifuge speed is 1000～2000 revs/min;
Centrifugate air distillation under 260～300 DEG C of conditions of temperature in described step 6).
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| JP6878407B2 (en) * | 2016-03-17 | 2021-05-26 | 日鉄ケミカル＆マテリアル株式会社 | Manufacturing method for artificial graphite electrodes |
| CN107099327A (en) * | 2017-06-27 | 2017-08-29 | 上海蓝科石化环保科技股份有限公司 | A kind of biomass coke tar pretreatment purification method and system |
| CN108342212B (en) * | 2018-01-23 | 2019-04-12 | 陕西煤业化工集团神木天元化工有限公司 | Handle the method and system of slag inclusion coal tar |
| CN115029801A (en) * | 2022-06-13 | 2022-09-09 | 中国科学院山西煤炭化学研究所 | Method and device for high-temperature centrifugal filtration continuous spinning of spinnable asphalt |
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